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目的建立了超高效液相色谱串联质谱法(UPLC-MS/MS)测定全血中甲哌啶的方法。方法样品血经pH=8氨水稀释后,涡旋离心,上清液过混合型弱阳离子交换柱(Oasis WCX)进行纯化,采用UPLC-MS/MS检测。质谱检测采用正离子扫描,多反应离子监测模式(MRM)。以甲哌啶母离子114.098(m/z)和子离子58.078(m/z)及98.215(m/z)定性、定量。结果加标回收率在65%~75%。在S/N≥3的情况下,检出限为0.3ng/mL。结论实验结果证明该方法灵敏度高,分析速度快,操作简便,适宜应用于法庭科学领域中解决甲哌啶中毒案件的检测。
Objective To establish a method for the determination of mepiperidine in whole blood by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS). Methods The blood samples were diluted with ammonia solution (pH = 8), vortexed, supernatant mixed with weak cation exchange (Oasis WCX) and purified by UPLC-MS / MS. MS detection using positive ion scan, multi-reactive ion monitoring mode (MRM). Methionine precursor 114. 988 (m / z) and the daughter ions 58.078 (m / z) and 98.215 (m / z) qualitative and quantitative. Results The spiked recoveries ranged from 65% to 75%. In the case of S / N≥3, the detection limit was 0.3 ng / mL. Conclusion The experimental results show that the method has high sensitivity, fast analysis speed and easy operation. It is suitable for the detection of mepidoxoxicosis cases in forensic science.